Removable absorbing agent unit for gas analyzers



2 Sheets-Sheet 1 c. A. SPRAGUE Filed Aug.. 5o, 1959 Feb..23, 1943.

REMOVABLE ABSORBING GENT UNIT FOR GAS ANALYZERS Feb. 23, 1943. C A .SPRAGUE' 2,312,285 F REMOVABLE ABSORBING AGENT UNIT FOR GAS ANALYPZERS Filed Aug. 3o, 1939 A 2 sheetssheet 2 l INVENTOR. C//Amfs A. .5m/1605.

.ATTORNEYQ Patented Feb. 23, 1943 REMOVABLE ABSORBING AGENT UNIT FOR GAS ANALYZERS Charles A. Sprague, Michigan City, Ind., assignor to The Hays Corporation, Michigan City, Ind.,

a corporation of Indiana Application August 30, 1939, Serial No. `292,573

9 Claims.

This invention relates to improvements in removable absorbing agent unit for gas analyzers, and more particularly to a unit containing phosphorus and adapted primarily for an oxygen analyzer.

The value of phosphorus as an absorbing agent for oxygen is well known. However, no practical manner for the use thereof in a gas analyzer of the Orsat type has ever been known heretofore. Consequently, it has generally been necessary in order'to obtain a measure of oxygen content in a gas, to use a less dangerous absorbing agent such as pyrogallic acid, which will absorb oxygen and some other constituent of the gas, such as carbon dioxide. At the same time that one sample of the gas is being analyzed as the aforesaid, another sample of the same gas is analyzed by the use of an absorbing agent, for the carbon dioxide only, such as caustic soda. A comparison of the results obtained and a computation of the difference in the two readings. gives the oxygen content. This method is naturally subject to the disadvantages of a double operation together with the necessity of mathematical computation.

The phosphorus is very dangerous to handle and this danger is one factor which has prevented its use in Orsat analyzers heretofore. Another factor which has made the use of phosphorus in gas analyzers diii'icult is the rapid formation of phosphorous pentoxide (P205) which coats the phosphorus and must be Washed away in order to maintain full absorptive properties of the phosphorus.

Therefore it is the primary object of this invention to provide novel and simple means to facilitate the use of phosphorus as an absorbing agent in a gas analyzer.

A further object is to provide a gas analyzer utilizing phosphorus as an absorbing agent, wherein provision is made to avoid the absorption-retarding effect of corrosion of the phosphorus, and wherein a simple apparatus to facilitate recharging with the phosphorus is provided.

A further object is to provide a container for an absorbing agent such as phosphorus, which may readily be applied to and removed from a gas analyzer by an operator in substantially the same condition in which the container is received from the manufacturer, and without necessity of opening the container or handling the phosphorus.

A further object is to provide a container for a gas absorbing agent with attachment means associated therewith, which means is of a character adapted for attachment of the container to either a gas analyzer or a shipping container without exposing said agent to manual contact.

A further object is to provide a nove1 container for phosphorus by means of which the same may be immersed in water while being shipped.

A further object is to provide a phosphorous container adapted to be inserted in a gas analyzer, and provided withmeans for feeding the phosphorus to a position of maximum eiciency for absorption as necessary in use thereof.

Other objects will be apparent from the description and appended claims.

In the drawings:

Fig. 1 is a side elevation of the upper portion of a gas analyzer having the casing portion thereof shown in section.

Fig. 2 is a side elevation of the lower portion of the gas analyzer, with parts shown in section.

Fig. 3 is a vertical sectional view of a shipping container for my improved absorbing agent unit and illustrating the latter in operative position in said casing.

Fig. 4 is a vertical sectional detail view of my absorbing agent unit illustrating the manner in which the same is mounted in the analyzer.

Fig. 5 is an enlarged top plan View of the plate of my unit which mounts the absorbing agent.

Fig. 6v is a vertical sectional view taken on line 6 6 of Fig. 5.

Fig. 7 is a fragmentary diagrammatic view of the analyzer illustrating the measuring chamber thereof, and associated parts.

Referring to the drawings, which illustrate the preferred embodiment of my invention, the numeral II'I indicates the casing of a gas analyzer from which depends a bracket II which in turn supports a casing I2 therebelow.

On top of the casing IU is mounted an aspirator I3 having a suitable valved water intake I4, and a gas intake I5. .Within casing I0 is mounted a standpipe I6 communicating with aspirator I3. standpipe I6 includes a laterally projecting portion I1 at its lower end, and a laterally projecting portion I8 adjacent its upper end.

A water tank I9 is mounted within the casing I0 spaced above portion I1 of the standpipe. Within the tank I9 is Xedly mounted a burette 20. The burette is interposed in a gas passage system best illustrated in Fig. 7, wherein a conduit 2I projects downwardly ,from the lower end of the burette and into the standpipe portion I1. A conduit 22 extends vertically upwardly from the top of the burette. A conduit 23 branches from convpoint of connection of conduits 23 and 24; and

conduit 25 joins conduit 2I above the point; of; connection of said conduits 23rand24. A syphon.` 28 has one leg thereof communicating with the standpipe I6, and the other leg 29 thereof passing through the bottom of casing I9 and into the top of lower casing I2. The bight or upper portion 39.0f syphon 28 projects slightly above the level` of the upper end of standpipe projection I3. A,

secondsyphon 3l is positioned within casing I2V with its upper portion 32 positioned adjacent' to the level of the lower portion ofsyphon run 29,v and has a discharge run 33 opening below the, bottom of casing I2.

An absorption chamber 35%, best illustrated in Fig. 4, is mounted within water chamber I9, saidl absorption chamber being open at its lower end. A compression chamber 35 isv placed in communi-i cation with water. chamber I9 and has an open ended calibrating tube 35 mounted vertically. within its top and adjustably positionedtherein. A syphon 31 has one leg thereof within chamber 35 adjacent tothe bottom thereof, and passes outwardly of said chamberv with its upper portion spaced below the top of Calibrating tube 35. The external vertical run 390i syphon 31 is connected with an extra supply tank 39 within the casing I0, and below the level of chamber 35. A conduit 40 comfmunicateswith the upper` end of chamber 39, andprojects downwardly to enter the casing# I2'. A bell 4| is positioned within casing I2` adjacent to the bottom thereof, with its bottom surface slightly. above the level with the inner endV of syphon 3l. Conduit MIV communicates, with bell 4I. AV bellv 42 is mounted in the upper end of standpipe portionv Iii-and is connected with the conduit 43 by means of a fitting 44. Conduit-43 extends to a suitable bellows (not shown) of the recording or indicating mechanism of the analyzer. A conduit 45 is connected by a suitable tting i5 with the upper end of compression chamber 35. Conduit 45 extends to and communicates with asecond bellows (not shown) of the indicatingV or recordingr mechanismv of the analyzer.

Referring now more specifically to the absorption chamber 34, best shown in Fig. 4, the same preferably comprises a cylindrical housing member open at both ends. At the upper end of the said housing member is mounted ahead 45A including a reduced neck portion 41,- and' an enlarged flange 4'8 adapted to overlie'the upper'end of the cylindrical member ofthe housing and to project outwardly therefrom, and a portion 49 extendingv within the upper end of the cylindrical housing. Head has a conical opening 59 formedvcentrally therein and tapering from the lower end thereof to a restricted diameter passage extending centrally through neck 41`. Head 49 is preferably welded to the cylindrical body 34. A gasket ring, 52 `fits around cylindrical body 34 and bearsagainst the lower surface of flange 49. A plurality of pins or studs 53 are phorus 55.

carried by the lower end of cylindrical housing 34 to project inwardly thereof. On these pins is normally supported a block 54 adapted for Vertical movement within the housing 34. Block 54 is preferably formed from Lucite or another material which will not corrode under the action of phosphorous or phosphoric acid. Block 54 has a plurality of sockets 55 formed therein and adapted to receive and support elongated sticks of phos- A plurality of apertures 51 are formed in the block throughout the same and extend entirelythrough the block.

A shaft 58 passes through a stuffing box 59 carried by the bottom of water chamber I9.

Shaft 5&1 isprOVided with a knurled hand grip 69 atits-lower end, hasa threaded engagement with the wall of water chamber I9 through which it passes, and bears against the bottom of block 54 at. the center of said block.

The absorpticnchamber unit is mounted in a suitable opening in the upper wall 6I of water chamber I9 and' issecured in operative relation'T to said water chamber by bolts 52'passing through the flanges 48 and into water chamber wall611 The operation of the device is as follows: AA small stream ofA water i's fed toaspirator I3V at intake I4 and exhausts into standpipe` I5; As' the water flows through the aspirator it draws' the gas to be analyzed from intake I5 through the aspirator I3' and thence through conduit 24. The water which enters, the standpipe fills the same within a certain interval, preferably `oper#k ating in cycles of' about' two minutes each', and' thus furnishes the motive power forthe'analyzer and controlsthe temperature and pressure'of'tl'ie gas sample. Thus, as the water rises in the standpipe I5, it passes upwardly in conduits 2I and 231 until it reaches the levelin conduitZI at which conduit 25.branches from conduit 2I all without interference to the continuous supplyvof gas by the aspirator in the following path: ConduitY 24 to conduit 23V to conduit 22 to burette 25'toconduit.2| and through to conduit 25Y to atmosphere. Thereafter as the water continues to rise in the standpipe and: in conduits 2| and 23;,the.con duits 24 and 25' are shut offv and a sample of'gas is trapped' in the burette fwheny the water in conduit 2'I reaches the level at which conduit 26 branches from conduit 2l. During this time the gascis forced into the atmospheric bag 21. to be measured at atmospheric pressure. When the water reaches a levelcompletely sealing tjhe connection between the conduits 2l and" 2*,rthere remainsA within the'burette or measuring chamber 20', a sampleof gas of a Aquantity accurately measured at atmospheric pressure. Hence' the basis for an accurate determination of oxygen absorptionV in terms of percentagel of'volume. is provided.

As the water continues, to rise in the standpipe, and also conduits 2|, 23 andassociated conduits, includingmeasuring chamber 29; the measured sample of gas is forced outwarddly through conduit 22 which extends upwardly from water chamber I9 to a level-slightly belowthe'upper endof' standpipe portion liand thence bends downwardly in a runy 53, which; is connected with the restricted opening 5I in neckV 41 of; the. measuring chamber. Aj removable connector 9'4" is threaded Y onV neck` 41'to accommodate disconnecf tion and-separation of conduit' Ii3'from` the absorbingA chamber; and? thereby facilitate"` applicationl and.'` removal of the' absorption chamber.

As thegas enterstheabsorption; chamber Vfrom conduit 63 it comes into intimate contact-,with the phosphorous sticks 56, thereby causing complete absorption of the oxygen component of the measinto the chamber I 9 and up into the compression chamber 35. The normal level of the water in compression chamber 35 is in the plane of the bottom edge of the inner leg of syphon 31. The Water is forced upwardly in compression chamber 35 until it reaches the level of the lower end of Calibrating tube 36 thereby sealing said tube.'

Hence any further rise of the water level inchamber 35 forces the air which is trapped in the upper end of said chamber through the fitting 46 and conduit 45 to the operating mechanism of the recorder or indicator with which the device is supplied.

The positioning of the portion I8 of the standpipe to extend above the upper end of conduit lassembly 22-63, provides a certain time lag between the time at which the gas is fully exhausted into the absorption chamber, and the time when the standpipe is completely filled. During this interval of time lag, the continued rise of water Within the standpipe creates a pressure within the bell 42 which is transmitted through fitting 44 and conduit 43 to a second bellows of the indicator or recorder for cooperative action with the bellows which is connected with conduit 45 as aforesaid. When the water in the standpipe reaches a level slightly above portion I3 thereof, and at upper portion 30 of syphon 28, the standpipe is automatically emptied lby lthe syphon. This allows the unabsorbed part of the gas sample in the compression chamber 34 to be pushed back into the measuring chamber 20, in prepara' tion for repetition of the cycle above described. A fresh stream of gas is supplied by conduit 24 and passes through the measuring chamber 26 for exhaust at conduit 25 for about one-halfminute before the water in the standpipe again reaches a level to close off the lower end of conduit 25. In this manner all gas residue from the preceding operation is swept out of the analyzer before a new sample is trapped. Also the water is permitted to rise in the absorption chamber 34 to the top thereof, to completely immerse the phosphorous sticks 56; thus washing the phosphorous pentoxide (P205) from the sticks.

As the water in the standpipe is discharged through syphon 28, it empties into the lower casing I2. This creates a pressure in the bell 4I which is transmitted through conduit 40 and forces some of the water out of supply tank 39 through tube 38 into compression chamber 35, thus assuring the maintenance of the desired water level in the waterchamber I9 and compression chamber 35. When the water in casing I2 reaches the upper end of said casing, it starts its own syphon 3| and is discharged at 33 to a suitable drain. The emptying of casing I2 releases the pressure on bell 4I, and causes any excess of Water above the bottom end of tube 31 in compression chamber 35 to be syphoned back into tank 39. The above operation constitutes self leveling of the analyzer to bring the water in chamber 35 to the level of the lower end of tube 3'I after each analysis, therefore eliminating all necessity for manual attention, and assuring positive accuracy.

The chamber 5 is preferably formed of such capacity thatit may wash all of the phosphorous pentoxide, formed in the full duration of operation ofthe device with one charge of phosphorous sticks, without creating too strong a solution of phosphoric acid within the chamber. In this way danger of corrosion of the tank and associated parte is substantially avoided. 'Ihe use of Lucite in the block 54 has also been made to avoid corrosion. Suitable means are provided in the chamber I9 for draining the same as required, preferably at the same time the analyzer is recharged with phosphorous.

The primary advantage of the invention resides in the character of the absorption chamber 34. In this connection note that the shaft 58 provides means for adjusting the vertical position of the block 54 carrying the phosphorous sticks. This assures proper positioning of the phosphorous sticks at the upper end of the absorption chamber at all times, so that the full absorptive value thereof may be obtained. In practice, it is found that the deterioration of the phosphorous sticks incident to the formation of phosphorous pentoxide during an analyzer operation, is such that an adjustment of shaft 58 is generally required about once a day when used with a continuously operated recording type of analyzer as herein de.`

scribed. 'The conical formation of the interior tapered opening 50 in the head 46 of the absorption chamber is so designed and proportioned that, as the sticks of phosphorous 56 are pressed thereag-ainst by operation of shaft 58 aforesaid, said sticks will maintain their operative position and afford maximum exposed surfaces for the absorption operation.

When the sticks have been used to maximum permissible measure, determined by maximum possible adjustment of block 54 upwardly in casing 36, the absorption chamber may be removed as a unit by disconnecting fitting 64 from conduit 63, and by removing the screws 62. The absorption chamber can then be lifted bodily out of the water chamber I9, during which time the water is permitted to drain from housing 34 through passages 5l in block 54, thereby eliminating possibility of contact by the operator with any of the phosphoric acid formed in said water chamber I9 as aforesaid. It will also .be seen that as chamber 34 is lifted out of chamber I9, block 54 will slide downwardly in chamber 34 to rest on the pins 53, which positively hold said block 54 vand the residue of the phosphorous sticks 56 carried thereby within the chamber 34. Hence the operator does not have to handle the phosphorous sticks 56 at any time, and said sticks are in fact so guarded and shielded that it is impossible for the operator to touch the same.

The problem of disposal of the residue of the gas absorbing agent, such as phosphorous, is one which only such concerns or suppliers as have special equipment are in condition to solve; and hence it is desirable to provide some means by which the residue of the absorbing agent may be shipped by the user to the supplier of the phosphorous. For this purpose, I have provided the shipping container best illustrated in Fig. 3. This container comprises an outer casing 65 which is open at its upper end and is preferably exterior- 1y screw threaded to receive and mount a sealing cover or cap 66. An inner container 67 is positioned within the container 65, and has an outwardly extending flange 68 formed at its upper end and substantially below the upper end of chamber 65. The flange 68 is of an outer diameter to fit snugly in casing 65 and 'serves to position-the-inner chamber 61 in spaced relation the, outerE chamber 65 and` against" lateralmovement.` Theabsorbing chamber 34fis1adapt-redto be 'positioned Within the inner cham-berl'l,

with its flange 43 bearing upon ange-68 ofinner chamber 6,1, and preferably bolted thereto-at 69:

A -cap -10 is threaded on the reduced neck 41 of head 46 of the absorption chamber to seal theA upperendof said chamber. Inner'chamber- 61 spreferably lledwith water in which the phosphorous sticks are immersed in transit. It will thus be seen that a safeandsimple sealed con-4 tainer is provided byv means of which the absorption chamber 34, with either anew oran exhausted charge of phosphorous sticks, may be shipped. Ther water Withinchamber 61 protectsl the phosphorous sticks from atmosphere While- Within the shipping container, thus preventing-A cor-rosion of the phosphorous and-rendering the container safe to handlers. The cap 10, serving as it does to seal the upper end of reduced passage 5| in neck 41, prevents entry of air through said'passage in the event the Water level is not high enough to completely immerse the phosphorous sticks, as in shipping anew charge;

The only requirement for special care on the part of the operator of an instrument providedwith my improved' phosphorous cartridge asaforesaid, exists inA connection with the operation of. draining the Water chamber l5 periodically to exhaust therefrom the phosphoric acidl which frms'therein. The cartridge itselfis of such character that only by willful tampering on the himself to-r par-t ofthe operator can he expose contact with the phosphorous-sticks. A further important advantage of the construction is that the apertured construction of the blockv 54' permits the'free passage or flow of Water through theI absorption chamber or cartridge unit in the `uring ka gas sample and thence shifting said* chamberA sample',` comprising anabsorption adapted to be carried by: and immersed in said container, means for supporting an absorbing agentV in said chamber, said chamber having openings Vforent-ry `of water thereinl +o-immerse said-agent, other attachment' means carried by said-chamber `for detachably connecting saidl chamber to said measuring means, other attachment means carried-'by said chamber for. detachablysecuring said chamber to saidcontainer;

saidattachment means accommodating removal.-

oi'- said absorption chamber andits contents from` the-a-nalyaer.; as a-unit-in whichnsaid--agent is fully-confined', andmeans-for adjustablyposi-` tioning said agent supporting means in,` saidchamber. v

2. A removable.- absorption unit for a. gas analyzer comprisinga-chamber-,-andr a carrier in` saidchamber for supporting. elements of gasl' absorbing-material ofpredetermined shape inpredetermined-spaced relation to each other, saidcarrier having a pluralityof restricted passagesv therethrough and being adjustable in said chamber, said chamber having an interior contoured` portion against which the-free portions of saidelements p-ress tomaintain the same-in operative` relation.-

3. An absorption unit for a gas analyzer comprising-a chamber open'at'one end and havinga-restrictedopening at itsI opposite end, a member slidable in said chamber having a pluralityr of sockets each adapted to receive one end of anelongated stick of phosphorus, said member having a plurality ofv restricted passages therethrough spaced from each other and fromsaid sockets, and means for retaining said member in said chamber.

4. The construction deiined in-claim 3, Wherein the inner contour of said chamber at the endthereof having saidV restricted-opening is tapered and adapted for abutment of the free end of said sticks thereagainst.

5. The combination with a casing open at one end and containing a gas absorbing agent, of a container having a water containing compartment receiving the open ended portion-of saidcasing, said casing-having a marginal projectingange overlying-themarginl of said compartment to seal the same.

6.- 'Ihe combination with a casing fora gas absorbingagent which is open at one-end and-- has a marginal projecting flangeatits opposite' end,'-ofa containerA having a reduced-dimension Water compartment at its lower end dened Aby an inwardly projecting shoulder on' which saidange seatswith theopen endof the casing -inl said compartment.

7. In combination, a casing for a gas absorb-y ing agent having aneck at one end and open at its oppositeend, said necklhaving a bore the-re-v through opening into the interior ofsaid-casing, a marginal ange projecting from said casing-at4v the base of said'neck, a container having areduced dimension Waterv chamber at-its lower endV dened by a shoulderlon which saidflange seats with the open end of' the casing'in said compartment, and a-cover sealing said container.

8.1 The combination deiined in claim '7, and means-fordetachably securing said ange'to said shoulder.

9.'The combination* defined' in claim 7, and means for sealing said-.neck bore.

CHARLES A. SPRAGUE. 

